A gas-liquid chromatographic (GLC) procedure is presented for the separation and quantitative determination of sucrose, lactose, maltose, and glucose in commercial confectionery products. By converting reducing sugars to oximes and then forming trimethylsilyl ethers of these compounds and separating them on a 6 ft × 4 mm id glass column packed with 2% OV-17 on 100—120 mesh Supelcoport, single peaks were obtained for each of the sugars. Results for sugars present in samples at levels of 5% or more are within 2.8%, on the average, of results obtained by polarization measurements. The data also compare favorably with others in the literature on similar products analyzed by other GLC procedures that do not involve oxime formation.